研究论文 RESEARCH PAPER

固相萃取结合液相色谱-串联质谱技术同时测定饲料中氯苯那敏和溴苯那敏含量

  • 管鑫 ,
  • 索德成 ,
  • 肖志明 ,
  • 王石 ,
  • 冯玉超 ,
  • 梁英 ,
  • 樊霞
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  • 1. 中国农业科学院农业质量标准与检测技术研究所, 北京 100081;
    2. 黑龙江八一农垦大学, 大庆 163000
管鑫(1995—),男,山东诸城人,硕士研究生,从事饲料质量安全监测技术研究。E-mail:1370300735@qq.com

收稿日期: 2022-05-17

  网络出版日期: 2022-12-15

基金资助

国家“十三五”重点研发计划(2019YFE0103800);推荐性国家标准计划项目(20214594-T-469)

Simultaneous Determination of Chlorpheniramine and Brompheniramine Contents in Feed by Solid-Phase Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

  • GUAN Xin ,
  • SUO Decheng ,
  • XIAO Zhiming ,
  • WANG Shi ,
  • FENG Yuchao ,
  • LIANG Ying ,
  • FAN Xia
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  • 1. Institute of Agricultural Quality Standards and Testing Technology, Chinese Academy of Agricultural Sciences, Beijing 100081, China;
    2. Heilongjiang Bayi Agricultural University, Daqing 163000, China

Received date: 2022-05-17

  Online published: 2022-12-15

摘要

本试验旨在建立一种固相萃取结合液相色谱-串联质谱技术同时测定饲料中氯苯那敏和溴苯那敏含量的方法。饲料样品用1%甲酸乙腈溶液提取,经混合型阳离子固相萃取柱(MCX)净化,采用液相色谱-串联质谱测定,以0.1%甲酸溶液(A)-乙腈(B)为流动相,梯度洗脱,C18色谱柱分离。通过使用不同饲料制备基质添加标准曲线,氯苯那敏和溴苯那敏含量在1.0~100.0 ng/mL内线性关系良好(R2>0.995 0);方法检出限为0.3 μg/kg,定量限为1.0 μg/kg;氯苯那敏和溴苯那敏在3个添加水平(1.0、10.0、100.0 μg/kg)下的平均回收率为85.8%~108.4%,相对标准偏差(RSD,n=6)<15%。该方法前处理简单,操作方便,适用于饲料中氯苯那敏和溴苯那敏含量的同步测定。

本文引用格式

管鑫 , 索德成 , 肖志明 , 王石 , 冯玉超 , 梁英 , 樊霞 . 固相萃取结合液相色谱-串联质谱技术同时测定饲料中氯苯那敏和溴苯那敏含量[J]. 动物营养学报, 2022 , 34(12) : 8097 -8107 . DOI: 10.3969/j.issn.1006-267x.2022.12.056

Abstract

This study aimed to establish a method for simultaneous determination of chlorpheniramine and brompheniramine contents in feed by solid-phase extraction combined with liquid chromatography-tandem mass spectrometry. Feed samples were extracted with 1% formic acid in acetonitrile solution, purified by MCX solid-phase extraction cartridge, and measured by liquid chromatography-tandem mass spectrometry, using 0.1% formic acid solution (A)-acetonitrile (B) as mobile phase, gradient elution, C18 column separation. By using different feeds to prepare the matrix addition standard curve, the linear relationship between chlorpheniramine and brompheniramine was good in the range of 1.0 to 100.0 ng/mL (correlation coefficient >0.995 0); the detection limit of the method was 0.3 μg/kg, and the limit of quantification was 1.0 μg/kg. The average recoveries of chlorpheniramine and brompheniramine at three spiked levels of 1.0, 10.0 and 100 μg/kg were 85.8% to 108.4%, and the relative standard deviation (RSD, n=6) <15%. The method is simple in pretreatment and convenient in operation, and is suitable for the simultaneous determination of chlorpheniramine and brompheniramine in feed.

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